Sodium Hydroxide → 7-Benzyl-1-tert-butoxycarbonylaminomethyl-2-oxa-7-azabicyclo[3.3.0]octane

HRID 53877ノート

反応式

HRID 53877 の反応式
[OH-:1].[Na+].[NH2:3][CH2:4][C:5]12[CH2:12][N:11]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:10][CH:9]1[CH2:8][CH2:7][O:6]2>O.C(O)(C)(C)C>[CH2:13]([N:11]1[CH2:12][C:5]2([CH2:4][NH:3][C:7]([O:6][C:5]([CH3:12])([CH3:9])[CH3:4])=[O:1])[CH:9]([CH2:8][CH2:7][O:6]2)[CH2:10]1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 15380948HCID 15380948、化合物

生成物 1

HCID 217047517-Benzyl-1-tert-butoxycarbonylaminomethyl-2-oxa-7-azabicyclo[3.3.0]octane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6386tert-Butanol溶媒

実験手順

2 g of NaOH in 45 ml of water are added to 10.4 g (44.7 mmol) of 1-aminomethyl-7-benzyl-2-oxa-7-azabicyclo[3.3.0]octane in 56 ml of tert-butanol, and 10.2 g (47 mmol) of di-tert-butyl pyrodicarbonate are then added dropwise. The mixture is stirred at room temperature for 15 hours, and then extraction with chloroform, drying over potassium carbonate, concentration and distillation are carried out. Yield: 12.2 g (82% of theory) Boiling point: 170° C./0.15 mbar The product is 94% pure by gas chromatography.

後処理

  1. additionare then added dropwise
  2. extractionextraction with chloroform
  3. dry with materialdrying over potassium carbonate, concentration and distillation

出典と根拠

ORDレコード
ord-c59503dc4a714864914894ff6abdeeeb
出典データセット
uspto-grants-1997_04
特許番号
US05621105

反応ノート

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